CN115608318A - Reed biochar material synthesized by phosphoric acid activation modification - Google Patents
Reed biochar material synthesized by phosphoric acid activation modification Download PDFInfo
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- CN115608318A CN115608318A CN202211151334.XA CN202211151334A CN115608318A CN 115608318 A CN115608318 A CN 115608318A CN 202211151334 A CN202211151334 A CN 202211151334A CN 115608318 A CN115608318 A CN 115608318A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/14—Paint wastes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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Abstract
The invention discloses a reed biochar material synthesized by phosphoric acid activation modification, which takes reed as a carbon source and forms a biochar mesoporous material with a developed pore structure after phosphoric acid activation treatment; the preparation method of the reed biochar material comprises the following steps: s1, cleaning reed raw materials, drying cleaned reeds for 12-24 hours at the temperature of 30-50 ℃, and crushing the dried reeds; s2, adding 10-30 ml of phosphoric acid solution with the mass concentration of 30-50% into a beaker, adding 3-9 g of the reed crushed in the step S1 into the beaker, and soaking for 5-12 h; the method for preparing the biochar material by using the reed and the phosphoric acid as raw materials has the advantages of simple process route, convenience in operation, environmental friendliness, cleanness, wide raw materials, low price and convenience in realizing industrial production.
Description
Technical Field
The invention relates to the technical field of industrial wastewater treatment and environment functional materials, in particular to a reed biochar material synthesized by activating and modifying phosphoric acid.
Background
With the rapid development of industries such as printing and dyeing, chemical industry and pharmacy, the treatment problem of industrial wastewater becomes a research hotspot, the adsorption method attracts great attention in wastewater treatment because of high speed and high efficiency, wherein the activated carbon has a highly developed pore structure and a huge specific surface area, and is an important adsorbent.
The reed is a perennial plant, aquatic or marsh, belongs to non-zonal vegetation, is not limited by zonal conditions in growth, can grow nationwide, is widely distributed and rich in resources, has developed ventilating tissues, has remarkable purifying effect on eutrophic water, is widely applied to the field of water treatment in recent years, is mostly used as emergent aquatic plants in the wetland, mainly adsorbs nitrogen, phosphorus and heavy metals in water when the reed is applied to sewage treatment, needs to be harvested in time, and has a difficult problem of plant treatment after harvesting.
Disclosure of Invention
The invention aims to provide a reed biochar material synthesized by phosphoric acid activation modification, which can be used as a high-efficiency adsorption material for sewage treatment.
In order to achieve the purpose, the invention provides the following technical scheme:
a reed biochar material synthesized by phosphoric acid activation modification is characterized in that reed is used as a carbon source, and is subjected to phosphoric acid activation treatment to form a biochar mesoporous material with a developed pore structure.
The preparation method of the reed biochar material synthesized by phosphoric acid activation modification comprises the following steps:
s1, cleaning reed raw materials, drying cleaned reeds for 12-24 hours at the temperature of 30-50 ℃, and crushing the dried reeds;
s2, adding 10-30 ml of phosphoric acid solution with the mass concentration of 30-50% into a beaker, adding 3-9 g of the reed crushed in the step S1 into the beaker, and soaking for 5-12 h;
s3, taking out the soaked reeds in the step S2, putting the reeds into a drying box, preserving heat for 6-24 hours at the temperature of 40-80 ℃, then putting the reeds subjected to heat preservation into a carbonization furnace for carbonization, cooling the reeds subjected to carbonization to room temperature, and taking out the reeds;
s4, the reed processed in the step S3 is biochar, the biochar is washed for 3-5 times by deionized water, and then the biochar is placed into a drying box and dried for 12-24 hours at the temperature of 30-50 ℃;
and S5, grinding the biochar material dried in the step S4, and screening the ground biochar particles through a 200-mesh standard sieve to obtain the reed biochar material synthesized by the phosphoric acid activation method.
Preferably, the size of the crushed reed in the step S1 is controlled to be 200 μm-2 mm.
Preferably, the carbonization furnace in step S3 is a muffle furnace.
Preferably, the reed in step S3 is carbonized in a specific manner, in which the carbonization furnace is heated to 400-600 ℃ at a rate of 0.5-2 ℃/min, and the heating is stopped after the carbonization furnace is maintained for 1-3 hours.
Preferably, the reed dipped in the step S2 is activated by microwaves, wherein the microwave frequency is 1800 MHz-3000 MHz, and the microwave treatment temperature is controlled at 40-60 ℃.
Preferably, the biochar dried in the step S4 is placed in an ultraviolet radiation box for ultraviolet radiation modification.
Preferably, when the biochar obtained in the step S4 is subjected to ultraviolet radiation modification, an ultraviolet lamp with the wavelength of 280-190 nm, namely purple is adopted for ultraviolet radiationThe external radiation intensity is 300-600 mu W/cm 2 The irradiation time is 18-36 h.
Preferably, the reeds are emergent aquatic plant reeds after nitrogen and phosphorus are adsorbed by the wetland.
Preferably, the biochar mesoporous material is used for treating printing and dyeing wastewater.
Compared with the prior art, the invention has the beneficial effects that: the method has the advantages of reasonable structural design, convenient operation, simple process route, convenient operation, environmental protection, cleanness, wide raw materials, low price and convenient realization of industrial production, and uses the reed and the phosphoric acid as raw materials to prepare the biochar material; the biochar material prepared by the invention has mesoporous aperture, large specific surface area and high activity; the surface of the biochar material prepared by the invention forms a phosphorus-containing group after being activated by phosphoric acid, and the content of acidic oxygen-containing functional groups, particularly the carboxyl concentration, is high; the method utilizes emergent aquatic plant reed after nitrogen and phosphorus are adsorbed by the wetland, and the calcined synthetic charcoal material is used for adsorbing the printing and dyeing wastewater, so that the adsorption capacity is large, the service life of the material is prolonged, and the multifunctional application of the material is expanded.
Drawings
FIG. 1 is a BET plot of the phosphoric acid activated modified synthetic reed biochar material of example 1;
FIG. 2 is a pore size distribution diagram of a phosphoric acid activated modified synthetic reed biochar material of example 1;
FIG. 3 is a graph showing the adsorption effect of the phosphoric acid activated and modified synthetic reed biochar material of example 1 on AO 7.
Detailed Description
The invention will now be described in detail with reference to fig. 1-3, for the sake of convenience, the orientations described hereinafter being defined as follows: the up, down, left, right, and front-back directions described below correspond to the up, down, left, right, and front-back directions in the projection relationship of fig. 1 itself.
Example 1:
the reed biochar material is synthesized by phosphoric acid activation modification, and takes reed as a carbon source, and forms a biochar mesoporous material with a developed pore structure after phosphoric acid activation treatment, wherein the reed is emergent aquatic plant reed after nitrogen and phosphorus are adsorbed by a wetland, and the biochar mesoporous material is used for treating printing and dyeing wastewater.
The preparation method of the reed biochar material synthesized by phosphoric acid activation modification comprises the following steps:
s1, cleaning reed raw materials, drying cleaned reeds for 12 hours at the temperature of 30 ℃, and crushing the dried reeds, wherein the size of the crushed reeds is controlled to be 200-1200 mu m;
s2, adding 10ml of phosphoric acid solution with the mass concentration of 30% into a beaker, adding 3g of the reed crushed in the step S1 into the beaker, and soaking for 5 hours, wherein the BET diagram of the reed biochar material synthesized by phosphoric acid activation modification is shown in figure 1;
s3, taking out the reed soaked in the step S2, putting the reed into a drying box, preserving heat for 6 hours at 40 ℃, then putting the reed after heat preservation into a carbonization furnace for carbonization, wherein the carbonization furnace is a muffle furnace, the temperature of the carbonization furnace is increased to 400 ℃ at the speed of 0.5 ℃/min, the heating is stopped after the carbonization furnace is maintained for 1 hour, and the reed after carbonization is cooled to room temperature and then taken out;
s4, the reed processed in the step S3 is biochar, the biochar is washed for 3 times by deionized water, and then the biochar is placed into a drying box to be dried at the temperature of 30 ℃ for 12 ℃;
and S5, grinding the biochar material dried in the step S4, and screening the ground biochar particles through a 200-mesh standard sieve to obtain the reed biochar material synthesized by a phosphoric acid activation method.
And (3) activating the soaked reed in the step (S2) by using microwaves, wherein the microwave frequency is 1800MHz, and the microwave treatment temperature is 40 ℃.
And (5) placing the biochar dried in the step (S4) in an ultraviolet radiation box for ultraviolet radiation modification.
When the biochar obtained in the step S4 is subjected to ultraviolet radiation modification, an ultraviolet lamp with the wavelength of 280nm is adopted for ultraviolet radiation, and the ultraviolet radiation intensity is 300 mu W/cm 2 The irradiation time is 18h, and as shown in FIG. 2, the pore size distribution diagram of the reed biochar material synthesized by phosphoric acid activation modification is shown.
Example 2:
the reed biochar material is synthesized by phosphoric acid activation modification, and takes reed as a carbon source, and forms a biochar mesoporous material with a developed pore structure after phosphoric acid activation treatment, wherein the reed is emergent aquatic plant reed after nitrogen and phosphorus are adsorbed by a wetland, and the biochar mesoporous material is used for treating printing and dyeing wastewater.
The preparation method of the reed biochar material synthesized by phosphoric acid activation modification comprises the following steps:
s1, cleaning reed raw materials, drying cleaned reeds for 18 hours at the temperature of 45 ℃, and crushing the dried reeds, wherein the size of the crushed reeds is controlled to be 1200-2200 micrometers;
s2, adding 20ml of phosphoric acid solution with the mass concentration of 40% into a beaker, adding 6g of the reed crushed in the step S1 into the beaker, and soaking for 8.5 hours;
s3, taking out the soaked reed in the step S2, putting the reed into a drying box, preserving heat for 15h at the temperature of 60 ℃, then putting the reed after heat preservation into a carbonization furnace for carbonization, wherein the carbonization furnace is a muffle furnace, the temperature of the carbonization furnace is increased to 500 ℃ at the speed of 1.2 ℃/min, heating is stopped after the carbonization furnace is kept for 2h, and the reed after carbonization is cooled to room temperature and then taken out;
s4, the reed processed in the step S3 is biochar, the biochar is washed for 4 times by deionized water, and then the biochar is placed into a drying box and dried for 18 hours at the temperature of 40 ℃;
and S5, grinding the biochar material dried in the step S4, and screening the ground biochar particles through a 200-mesh standard sieve to obtain the reed biochar material synthesized by a phosphoric acid activation method.
And (3) activating the soaked reed in the step (S2) by using microwaves, wherein the microwave frequency is 2400MHz, and the microwave treatment temperature is 50 ℃.
And (5) placing the biochar dried in the step (S4) in an ultraviolet radiation box for ultraviolet radiation modification.
When the biochar obtained in the step S4 is subjected to ultraviolet radiation modification, an ultraviolet lamp with the wavelength of 240nm is adopted for ultraviolet radiation, and the ultraviolet radiation intensity is 450 mu W/cm 2 Irradiation time of 27h。
Example 3:
the reed biochar material is synthesized by phosphoric acid activation modification, and takes reed as a carbon source, and forms a biochar mesoporous material with a developed pore structure after phosphoric acid activation treatment, wherein the reed is emergent aquatic plant reed after nitrogen and phosphorus are adsorbed by a wetland, and the biochar mesoporous material is used for treating printing and dyeing wastewater.
The preparation method of the reed biochar material synthesized by phosphoric acid activation modification comprises the following steps:
s1, cleaning reed raw materials, drying cleaned reeds for 24 hours at the temperature of 50 ℃, and crushing the dried reeds, wherein the size of the crushed reeds is controlled to be 2200 mu m-2 mm;
s2, adding 30ml of phosphoric acid solution with the mass concentration of 50% into a beaker, adding 9g of the reed crushed in the step S1 into the beaker, and soaking for 12 hours;
s3, taking out the soaked reeds in the step S2, putting the reeds into a drying box, preserving heat for 24 hours at the temperature of 80 ℃, then putting the reeds subjected to heat preservation into a carbonization furnace for carbonization, wherein the carbonization furnace is a muffle furnace, the temperature of the carbonization furnace is increased to 600 ℃ at the speed of 2 ℃/min, heating is stopped after the carbonization furnace is kept for 3 hours, and the reeds subjected to carbonization are cooled to room temperature and then taken out;
s4, the reed processed in the step S3 is biochar, the biochar is washed for 5 times by deionized water, and then the biochar is placed into a drying box and dried for 24 hours at the temperature of 50 ℃;
and S5, grinding the biochar material dried in the step S4, and screening the ground biochar particles through a 200-mesh standard sieve to obtain the reed biochar material synthesized by a phosphoric acid activation method.
And (3) activating the soaked reed in the step (S2) by using microwaves, wherein the microwave frequency is 3000MHz, and the microwave treatment temperature is 60 ℃.
And (5) placing the biochar dried in the step (S4) in an ultraviolet radiation box for ultraviolet radiation modification.
When the biochar obtained in the step S4 is subjected to ultraviolet radiation modification, the ultraviolet radiation adopts the wavelength of 190nmThe ultraviolet radiation intensity of the ultraviolet lamp is 600 mu W/cm 2 The irradiation time was 36 hours.
Experimental example:
1. weighing 11 parts of 0.02g of the reed biochar prepared in example 1, and placing the reed biochar in 150mL conical flasks respectively;
2. adding 100mL of AO7 solution into each conical flask, wherein the initial concentration of the AO7 solution in each conical flask is 20, 40, 60, 80, 120, 160, 200, 280, 360, 480 and 600mg/L, and the initial pH value of the solution is 4;
3. then placing the conical flask into a constant temperature oscillator with the temperature of 298K, and oscillating for 4d at the rotating speed of 150 r/min;
4. after the adsorption in the conical flask is balanced, filtering by using a filter membrane of 0.45 mu m, and measuring the concentration of AO7 in the filtrate;
5. the adsorption capacity of reed biochar was 530mg/g as fitted to the Langmuir model shown in FIG. 3.
Claims (10)
1. A reed biochar material synthesized by phosphoric acid activation modification is characterized in that the reed biochar material takes reed as a carbon source and forms a biochar mesoporous material with a developed pore structure after phosphoric acid activation treatment.
2. The method for preparing a phosphoric acid activated modified synthetic reed biochar material according to claim 1, which comprises the following steps:
s1, cleaning reed raw materials, drying cleaned reeds for 12-24 hours at the temperature of 30-50 ℃, and crushing the dried reeds;
s2, adding 10-30 ml of phosphoric acid solution with the mass concentration of 30-50% into a beaker, adding 3-9 g of the reed crushed in the step S1 into the beaker, and soaking for 5-12 h;
s3, taking out the soaked reeds in the step S2, putting the reeds into a drying box, preserving heat for 6-24 hours at the temperature of 40-80 ℃, then putting the reeds subjected to heat preservation into a carbonization furnace for carbonization, cooling the reeds subjected to carbonization to room temperature, and taking out the reeds;
s4, the reed processed in the step S3 is biochar, the biochar is washed for 3-5 times by deionized water, and then the biochar is placed into a drying box and dried for 12-24 hours at the temperature of 30-50 ℃;
and S5, grinding the biochar material dried in the step S4, and screening the ground biochar particles through a 200-mesh standard sieve to obtain the reed biochar material synthesized by a phosphoric acid activation method.
3. The preparation method of reed biochar material according to claim 2, wherein the preparation method comprises the following steps: in the step S1, the size of the crushed reed is controlled to be 200 mu m-2 mm.
4. The preparation method of reed biochar material according to claim 2, wherein the preparation method comprises the following steps: and the carbonization furnace in the step S3 is a muffle furnace.
5. The preparation method of reed biochar material according to claim 2, wherein the preparation method comprises the following steps: the concrete carbonization mode of the reed in the step S3 is that the carbonization furnace is heated to 400-600 ℃ at the speed of 0.5-2 ℃/min, and the heating is stopped after the temperature is kept for 1-3 h.
6. The preparation method of the reed biochar material as claimed in claim 2, wherein the preparation method comprises the following steps: and (3) activating the soaked reeds in the step (S2) by using microwaves, wherein the microwave frequency is 1800 MHz-3000 MHz, and the microwave treatment temperature is controlled at 40-60 ℃.
7. The preparation method of reed biochar material according to claim 2, wherein the preparation method comprises the following steps: and (5) placing the biochar dried in the step (S4) in an ultraviolet radiation box for ultraviolet radiation modification.
8. The preparation method of the reed biochar material as claimed in claim 7, wherein the preparation method comprises the following steps: when the biochar obtained in the step S4 is subjected to ultraviolet radiation modification, an ultraviolet lamp with the wavelength of 280-190 nm is adopted for ultraviolet radiation, and the ultraviolet radiation intensity is 300-600 mu W/cm 2 The irradiation time is 18-36 h.
9. The phosphoric acid activated and modified synthetic reed biochar material as claimed in claim 1, wherein the reed is an emergent aquatic plant reed after nitrogen and phosphorus are adsorbed by the wetland.
10. The application of the synthetic reed biochar material activated and modified by phosphoric acid as claimed in claim 1, is characterized in that the synthetic reed biochar material is applied to treatment of printing and dyeing wastewater.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117160405A (en) * | 2023-09-11 | 2023-12-05 | 山东建筑大学 | Calcium chloride activated adsorption-catalytic oxygen oxidation characteristic biochar, preparation method and application |
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| CN110327882A (en) * | 2019-07-11 | 2019-10-15 | 江西省科学院 | The preparation method and application of multidigit activation and modified reed-south reed charcoal |
| CN114307965A (en) * | 2022-01-18 | 2022-04-12 | 武汉科技大学 | Modification development and application of straw biochar |
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- 2022-09-21 CN CN202211151334.XA patent/CN115608318A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20140162873A1 (en) * | 2012-07-11 | 2014-06-12 | South Dakota State University | Materials and methods for production of activated carbons |
| CN108892342A (en) * | 2018-07-17 | 2018-11-27 | 苏州科技大学 | A kind of preparation method of the fixed composite material of Sediments heavy metal |
| CN108970583A (en) * | 2018-08-07 | 2018-12-11 | 沈阳环境科学研究院 | A kind of preparation method of reed base charcoal adsorbent material |
| CN109110863A (en) * | 2018-09-20 | 2019-01-01 | 湖南大学 | Utilize the method for fortimicin in chemical activation/micro-wave digestion activation biological carbon materials removal water body |
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| CN117160405A (en) * | 2023-09-11 | 2023-12-05 | 山东建筑大学 | Calcium chloride activated adsorption-catalytic oxygen oxidation characteristic biochar, preparation method and application |
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